CN104927816A - Environmental-friendly organic profile control agent and preparation method and use thereof - Google Patents
Environmental-friendly organic profile control agent and preparation method and use thereof Download PDFInfo
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- C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
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- C09K8/508—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
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Abstract
The invention relates to an environmental-friendly organic profile control agent. The environmental-friendly organic profile control agent comprises partially hydrolyzed polyacrylamide, a crosslinking solution, a ternary metal compound particles, an accelerant, additives, modified bentonite, auxiliaries, a complexing agent, polymetal silicate and water. The invention further provides a preparation method and use of the profile control agent. According to the profile control agent provided by the invention, the most excellent performances are obtained by proper selection of the components, a unique process of the preparation method and the like, so that the profile control agent has good application prospect and industrial potential in the field of petroleum industry.
Description
Technical field
Be used for improving amendment composition and method of making the same and the purposes of petroleum products in the present invention relates to a kind of oilfield exploitation and developing, relate more particularly to a kind of environmental protection organic profile control agent and preparation method thereof and purposes, belong to oil gas development technology field.
Background technology
In the oil production of field of oil development, along with the prolongation of life of oilwell, aquifer yield increase be the common problem run into, and use amendment especially plugging agent can significantly improve oil recovery, thus increase economic efficiency, and oil well life-span and the exploitation time limit can be increased to greatest extent.
Along with the progress of science and technology, countries in the world all develop the various water-plugging techniques adapting to respective geology characteristic, such as mechanical process, chemical method.Wherein, chemical method be most widely used, the most significant method of effect.
At first, amendment is only simple grout, then in succession develops oil based cement, milk of lime, reactive resin, active viscous crude etc.Enter into the eighties of last century 70-80 age, water-soluble polymers, gel etc. start in field use, and achieve unusual effect.
At present, profile control and water plugging is a kind of water-plugging technique the most remarkable and important, in the embody rule in oil field, the multiple profile control and water plugging technologies such as Weak Gels, colloidal dispersed gel, expanded granular, flexible particle are there is, these profile control and water plugging technologies have respective advantage, different geological conditions can be applicable to, thus be widely used.
But these profile control and water plugging technologies still more or less there is certain defect, such as specificity strong (universality is poor), high temperature resistance is more weak, abrasion resistance is poor, the property noted is poor, therefore, in order to the profile-controlling and plugging agent of development of new, people have carried out a large amount of further investigations, and achieve many achievements, such as:
CN1704559A discloses a kind of high strength easy and dissolves nanometer amendment, be applicable to the water blockoff of oil field high water-cut well, by 5-8% nano silicon oxide, the nano-sized iron oxide of 3-5%, the nano-calcium carbonate of 13-20%, the nano aluminium oxide of 5-10%, the ultra tiny cement of 20-30%, 1-3% sodium hydroxide, the iron complex salt of 1-2% and 30-50% water composition, after this plugging agent hydration and sclerosis hard as Behavior of Hardened Cement Paste and volume do not shrink, do not produce microfracture, chemical method dissolve after total overall reaction generate yellow transparent the aqueous solution and without residue, mobility is as water, effectively can solve the interim water blockoff of waterflooding oil field high water-cut well interlayer.
CN1673309A discloses a kind of expanding flow-gel profile-controlling agent, this amendment formula is: polymeric flocculant strength of solution 0.05-0.2%%, mix with the melamine-modified phenolic resin delayed crosslinker 0.05-0.8% of urine, the pH value of control gel reaction temperature 40-100 DEG C, solution system is 7.2-8.0.This profile-controlling and plugging agent has high water swellability (rate of expansion 1-3 doubly), mobility, high visco-elasticity, high deformability, delayed cross-linking capacity, also there is the characteristics such as intensity adjustability, auto repair capacity, shear resistant, salt tolerance, temperature tolerance, water-retentivity, adapt to the needs of the heavy dose of deep profile controlling water blockoff in oil field and transfer drive, profile control and water plugging is effective, should apply in oil field.
CN1827730A discloses one and automatically cracks particulated gel amendment of migrating again, it comprises following concrete component: polymer anti-salt temperature resistance polypropylene amine strength of solution 0.05-0.4%, flocculant addition 0.02-0.2%, modified polyester resin linking agent add-on 0.2-0.8%, ether of cellulose dispersion agent add-on 0.01-0.1%, by each component above-mentioned at temperature 60-90 DEG C, pH value is react under 7.2-8.0 to obtain, it has migration property again, swelling property, high visco-elasticity, delayed cross-linking capacity, the various features such as intensity adjustability, effectively can reach the object on shutoff stratum.
CN1944571A discloses a kind of single group liquid film type microcapsule deep amendment, it is made up of the composition of following mass percent: the yellow lemon of 5-30% water glass, 1-10 activator formaldehyde, 00.1-0.2% coating, 0.3-0.5% chelator acid citrate aluminium, 0.01-0.14% coagulant aids, surplus is water.Described liquid film type microcapsule deep water blocking agent take water glass as host, and formaldehyde is activator, can keep the advantage of general plugging agent, has again long, the plurality of advantages such as setting strength is high, gelling temp is controlled, construction technology is simple time of coagulation.
CN101440277A discloses a kind of selective profile control agent, it is made up of the raw material of following weight part: polyacrylamide 38-48 part, hexamethyl tetramine 49-65 part, N, N-methylene-bisacrylamide 2-4 part, Ammonium Persulfate 98.5 0.01-0.03 part, methacryloyloxyethyltrimethylammoniumchloride 3-6 part, hydroxypropyl oxygen methylcellulose gum 1-3 part, diethylenetriamine 6-15 part, the flowing of described selective water shutoff agent energy formation water produces larger resistance, water phase permeability is significantly reduced, and it is very little to the flow effect of crude oil, play the effect of the not stifled oil of water blockoff, obviously can improve the development efficiency of high-water-cut oil-producing well, improve crude production rate and oil recovery.
CN101712863A discloses a kind of water plugging agent for carbonatite, this plugging agent described is made up of the raw material of following weight part: cement 5-14 part, quartz 4-8 part, Flocculated Cement agent 0.1-0.5 part, density light-weight additive 4-11 part, spatial grid structure agent 1-2 part, water 72-74 part, described plugging agent splicing degree is strong, density is low, and be applicable to high temperature, the environment of the carbonatite oil well of high salinity, thus the environment not being suitable for high temperature and high salinity that in correlation technique, plugging agent exists can be solved, cementing property is poor, density is large, effectively cannot control water, improve the problem of oil recovery.
CN101892037A discloses a kind of novel salt-resistant gel selective water shutoff agent, mainly comprise: cationic polyacrylamide 0.54-0.64%, linking agent 0.8-1.6%, phenol 0.9-1.2%, conditioning agent 0.02-0.6%, NaCl 0-4%, surplus is water, and described selective water shutoff agent water plugging rate is greater than 95%, oil plugging rate is less than 30%, temperature resistance reaches 85 DEG C; Resistance to salinity (in sodium-chlor) the highest 4000mg/L, gel time are greater than 96 hours.
CN102134480A discloses a kind of plugging agent, comprises slag powders 66-70 part, kaolin 3-7 part, calcium oxide 3-7 part, calcium carbonate superfine powder 8-12 part, Calucium Silicate powder 6-10 part, water glass 1-3 part, Polyanionic Cellulose 0.5-1.5 part and short velveteen 0.5-2 part.After this plugging agent is extruded onto zone of interest termination of pumping, just the thickness state of ot-yet-hardened is become by runny suspensoid, thus can effectively reside in shutoff position and not miss, thus improve shutoff success ratio, be introduced into height after entering stratum and ooze out water layer, short velveteen is combined with gelatinous mass water glass, form spatial grid structure and reduce high rate of permeation of oozing out water layer, energy better solutions has decided the interlayer permeability contrast of water layer, make whole water-yielding stratum blocking radius consistent, overcome conventional plugging agent and differ the short drawback of the validity period that causes more greatly in different rate of permeation water-yielding stratum blocking radius, and in well temperature, same response of stratum under pressure, closely be cemented to an entirety, ultimate compression strength is high, realize the efficient shutoff of water-yielding stratum.
CN102304354A discloses a kind of amendment of field produces, this amendment is urinated air aldehyde resin delayed crosslinker, calcined soda for industry, Metha Amino Phenon and water by polymeric flocculant, dicyandiamide modified and is formed, and wherein the weight ratio of each component is: polymeric flocculant 0.08-0.2%; Dicyandiamide modified urine air aldehyde resin delayed crosslinker 0.18-0.25%; Calcined soda for industry 0.05-0.2%; Metha Amino Phenon 0.01-0.02%; All the other are water.Described plugging agent has certain mechanical blockage effect, oil effect taken by lasting mobile ponding, the effect of dynamic adaptation water, pressure vibration effect, washing oil, can meet the needs of the heavy dose of deep profile controlling water blockoff of oil field low-temperature reservoir and transfer drive.
CN102604608A discloses a kind of Water shutoff agent for extra-low permeability oil reservoir, and it is mixed by detergent, host, solidifying agent and water, and wherein, detergent is sulfonated petro-leum, fatty alcohol polyoxyethylene ether sulfate or nonionogenic tenside; Host is phenol and formaldehyde; Solidifying agent is carboxylic acid, sulfonic acid or ammonium chloride.This plugging agent can inject ultralow permeable reservoir smoothly, after blocking agent solidification, can generate the solid matter of high strength, closely cementing with rock, and without perviousness, aqueous phase breakthrough pressure>=35MPa, heatproof reach 150 DEG C, resistance to highly basic and strong acid, can meet rate of permeation and be less than 1 × 10
-3μm
2, pore throat radius R is less than the requirement of the extra-low permeability oil reservoirs water blockoff of 8 μm.
As mentioned above, although disclose the multiple amendment especially plugging agent that can be used for Petroleum finance field in prior art, but urgent demand is still existed for the manufacture and exploit of amendment that is novel and that have superperformance, this is for oil and gas development, especially experiencing high term and the secondary development of stepping into the oil field of degradation period is of great practical significance, is also the important leverage ensureing national oil safety.
Consider based on this, how to develop and a kind of there is novel organic profile control agent of the performances such as excellent heatproof, the property noted, abrasion resistance and preparation method thereof, study hotspot just in this field current and emphasis, this technical progress for petroleum prospecting and exploitation has very important industrial value and significance of scientific research, and this also just the basis that is accomplished of the present invention lean on and power place.
Summary of the invention
Based on above-mentioned shortcoming, the present inventor passes through and concentrates on studies, many defects that the profile-controlling and plugging agent in producing for existing Oil/gas Well shows, by further investigation, after having paid a large amount of creative works, thus obtain a kind of environmental protection organic profile control agent, and then complete the present invention.
Specifically, technical scheme of the present invention and content relate generally to following several aspect.
First aspect, the present invention relates to a kind of environmental protection organic profile control agent, described amendment comprises partially hydrolyzed polyacrylamide, crosslinker solution, ternary metal composite particles, promotor, additive, modified alta-mud, auxiliary agent, complexing agent, the many metal-salts of silicic acid and water.
In described environmental protection organic profile control agent of the present invention, with parts by weight, its concrete component concentration is as follows:
In described environmental protection organic profile control agent of the present invention, relate to composition " comprising ", both contained open " comprising ", " comprising " etc. and similar meaning thereof, also contains enclosed " by ... composition " etc. and similar meaning thereof.
In described environmental protection organic profile control agent of the present invention, the weight part of described partially hydrolyzed polyacrylamide is 0.2-1.5, such as, can be 0.2 part, 0.4 part, 0.6 part, 0.8 part, 1 part, 1.2 parts, 1.4 parts or 1.5 points.
Wherein, described partially hydrolyzed polyacrylamide is anion-polyacrylamide, and its molecular weight is 2,000 ten thousand-2,800 ten thousand, degree of hydrolysis is 20-30% and solid content is 97-99%; Most preferably its molecular weight is 2400-2450 ten thousand, degree of hydrolysis be 25-27% and solid content is 98%.
Described partially hydrolyzed polyacrylamide is known material in the art, and buy by multiple commercial channel, this is no longer going to repeat them.
In described environmental protection organic profile control agent of the present invention, the weight part of described crosslinker solution is 0.3-0.8 part, such as, can be 0.3 part, 0.5 part, 0.7 part or 0.8 part.
Described crosslinker solution prepares according to the method comprised the steps, its preparation method comprises the steps: in other words
S1: in the presence of an inorganic base, in reactor, a diisopropyl benzene and oxygen generation oxidizing reaction, obtain dicumyl peroxide; Then add acid, fully stir, obtain intermediate reaction product and acetone, removing acetone;
S2: add formalin in intermediate reaction product, react, has reacted rear removing water layer, then in residue system, adds organic solvent and water, stirs, obtain described crosslinker solution.
Wherein, in step sl, described mineral alkali can be in KOH, NaOH, sodium sulphite, sodium carbonate, sodium sulfate, salt of wormwood or sodium phosphate etc. any one, most preferably be sodium sulphite.
Wherein, in step sl, the mass ratio of described mineral alkali and a diisopropyl benzene is 0.1-0.3:100, such as, can be 0.1:100,0.2:100 or 0.3:100.
Wherein, in step sl, a diisopropyl benzene and oxygen react, and this reaction realizes, until reacted by continuing to pass into oxygen in reaction system.
Wherein, in step sl, the reaction times is not particularly limited, and such as, residual content by detecting raw material judges, this is the conventional detection means in chemical reaction, and this is no longer going to repeat them, and this time such as can be 30-60 minute; Temperature of reaction is 20-40 DEG C, such as, can be 20 DEG C, 30 DEG C or 40 DEG C.
Wherein, in step sl, the aqueous hydrochloric acid of described acid to be mass percent concentration be 10-20%, the amount of this aqueous hydrochloric acid is not particularly limited, but be preferably after abundant stirring subsequently no longer layering separate out acetone be advisable, one side like this can economize in raw materials, and can alleviate burden and the environmental influence of subsequent disposal on the other hand.
Wherein, in step s 2, the mass percent concentration of described formalin is 20-30%, such as, can be 20%, 25% or 30%.
Wherein, in step s 2, between in the formaldehyde in described formalin and step S1, the mol ratio of diisopropyl benzene is 1:1.5-2.5, such as, can be 1:1.5,1:2 or 1:2.5.
Wherein, in step s 2, the reaction times is 4-8 hour, such as, can be 4 hours, 6 hours or 8 hours; Temperature of reaction is 40-60 DEG C, such as, can be 40 DEG C, 50 DEG C or 60 DEG C.
Wherein, in step s 2, described organic solvent is the equal-volume mixture of acetone and ethanol, and this organic solvent (i.e. described mixture) is 1:2-3 with the volume ratio of described residue system, such as, can be 1:2,1:2.5 or 1:3.
Wherein, in step s 2, the water added and the volume ratio of organic solvent are 1:2.
In described environmental protection organic profile control agent of the present invention, the weight part of described ternary metal composite particles is 0.04-0.07 part, such as, can be 0.04 part, 0.05 part, 0.06 part or 0.07 part.
Wherein, described ternary metal composite particles prepares according to the method comprised the steps, its preparation method comprises the steps: in other words
(1) potassium chloride solution of the magnesium nitrate aqueous solution of 1mol/L, the aluminum sulfate aqueous solution of 1mmol/L and 1mmol/L is prepared respectively;
(2) in sodium phosphate aqueous solution, slowly add the NaOH aqueous solution, preparation NaOH concentration is 2mol/L and sodium phosphate concentration is the aqueous solution of 0.5mol/L;
(3) in the aqueous solution of step (2), add the magnesium nitrate aqueous solution of step (1), aluminum sulfate aqueous solution and potassium chloride solution in turn, after adding, Keep agitation 30-50 minute, obtains reacting slurry;
(4) by reacting slurry at 100-120 DEG C leave standstill slaking 3-4 hour, then naturally cool to room temperature, filter, deionized water fully wash 2-3 time, vacuum-drying, ground 300 mesh sieves, obtain described ternary metal composite particles.
Wherein, in step (3), the volume ratio of described magnesium nitrate aqueous solution, aluminum sulfate aqueous solution and potassium chloride solution is 2:1:2, and the volume ratio of the aqueous solution of the cumulative volume of these three kinds of aqueous solution and step (2) is 1:4-6, such as, can be 1:4,1:5 or 1:6.
In described environmental protection organic profile control agent of the present invention, the weight part of described promotor is 0.02-0.06 part, such as, can be 0.02 part, 0.04 part or 0.06 part.
Wherein, described promotor is the mixture of potassiumphosphate and Sodium salts humic acids, and both mass ratioes are 1:2.
In described environmental protection organic profile control agent of the present invention, the weight part of described additive is 0.08-0.12 part, such as, can be 0.08 part, 0.1 part or 0.12 part.
Wherein, described additive is Amino Trimethylene Phosphonic Acid four sodium, 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid four sodium or ethylene diamine tetra methylene phosphonic acid five sodium, most preferably is 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid four sodium.
In described environmental protection organic profile control agent of the present invention, the weight part of described modified alta-mud is 0.04-0.1 part, such as, can be 0.04 part, 0.06 part, 0.08 part or 0.1 part.
Wherein, described modified alta-mud prepares according to the method comprised the steps, its preparation method comprises the steps: in other words
I, wilkinite is calcined 20-30 minute at 500-600 DEG C, be then cooled to room temperature, and pulverize, grind, cross 300 mesh sieves, obtain wilkinite powder;
II, wilkinite powder, dimethyl dodecyl ammonium chloride and deionized water and stirring is even, at 50-60 DEG C, react 2-3 hour, then filter, vacuum-drying, obtain described modified alta-mud.
Wherein, in described Step II, the mass ratio of wilkinite powder, dimethyl dodecyl ammonium chloride and deionized water is 1:1.5-2.5:10-20, is preferably 1:2:15.
In described environmental protection organic profile control agent of the present invention, the weight part of described auxiliary agent is 0.08-0.15 part, such as, can be 0.08 part, 0.1 part, 0.12 part, 0.14 part or 0.15 part.
Wherein, described auxiliary agent is any one in ethoxyl methyl cellulose ether, hydroxypropyl methyl cellulose ether,
In described environmental protection organic profile control agent of the present invention, the weight part of described complexing agent is 0.1-0.14 part, such as, can be 0.1 part, 0.12 part or 0.14 part.
Wherein, described complexing agent is any one or mixture multiple arbitrarily in Sunmorl N 60S, ethylenediamine tetraacetic acid (EDTA), diethylene triaminepentaacetic acid(DTPA), oxine, nitrilotriacetic acid(NTA) or thiocarbamide, most preferably is nitrilotriacetic acid(NTA).
In described environmental protection organic profile control agent of the present invention, the weight part of the many metal-salts of described silicic acid is 0.05-0.09 part, such as, can be 0.05 part, 0.07 part or 0.09 part.
Wherein, the many metal-salts of described silicic acid prepare according to the method comprised the steps, its preparation method comprises the steps: in other words
(I) to mass percent concentration be 1-2% sodium silicate aqueous solution in add the aqueous sulfuric acid that mass percent concentration is 10-20%, to regulate pH=4-5, then at room temperature stir 10-20 minute, obtain acidic aqueous solution;
(II) in described acidic aqueous solution, add Tai-Ace S 150, zinc nitrate and titanium chloride, and stir, be then warming up to 45-55 DEG C with the temperature rise rate of 2 DEG C/min, stir 20-30 minute at such a temperature; Be warming up to 65-80 DEG C with the temperature rise rate of 6 DEG C/min again, stir 10-15 minute at such a temperature, finally leave standstill slaking 15-20 hour at such a temperature, drying, solidification, ground 300 mesh sieves, obtain the many metal-salts of described silicic acid.
Wherein, in step (II), the mol ratio of Tai-Ace S 150, zinc nitrate and titanium chloride is 1:1:2, and wherein the mole dosage sum of the three of aluminium element, zinc element and titanium elements is 4-5:1 with the ratio of the mole dosage of element silicon in water glass.
In described environmental protection organic profile control agent of the present invention, the weight part of described water is 20-40 part, such as, can be 20 parts, 25 parts, 30 parts, 35 parts or 40 parts.
Second aspect, the invention still further relates to the preparation method of above-mentioned organic profile control agent, and described method comprises the steps:
(1) partially hydrolyzed polyacrylamide of respective weight part, crosslinker solution, ternary metal composite particles, promotor, additive, modified alta-mud, auxiliary agent, complexing agent, the many metal-salts of silicic acid and water is taken respectively;
(2) Xiang Shuizhong adds partially hydrolyzed polyacrylamide, crosslinker solution for total weight parts 60-80%, ternary metal composite particles, promotor, additive, modified alta-mud, auxiliary agent, complexing agent and the many metal-salts of silicic acid successively, and stirring reaction 50-70 minute, obtain pre-gathering solutions;
(3) in described pre-gathering solutions, add the crosslinker solution of residuals weight part, and continue stirring reaction 20-40 minute, obtain environmental protection organic profile control agent of the present invention.
3rd aspect, the present invention relates to the purposes of above-mentioned organic profile control agent in oil production.
Contriver finds through research, described environmental protection organic profile control agent of the present invention has multiple excellent effect, and each composition environmental protection, safety, to environment toxicological harmless or negative effect, can be used for Petroleum finance, be particularly useful in oil production, petroleum industry has good industrial application potentiality and marketable value.
In sum, the invention provides a kind of environmental protection organic profile control agent, preparation method and its usage, described environmental protection organic profile control agent has many excellent properties such as good profile control effect, the property noted, abrasion resistance and heat resistance, has significant technique effect and application potential in field of petroleum exploitation.
Embodiment
Below by specific embodiment, the present invention is described in detail; but the purposes of these exemplary embodiments and object are only used for exemplifying the present invention; not any type of any restriction is formed to real protection scope of the present invention, more non-protection scope of the present invention is confined to this.
Crosslinker solution preparation example 1
S1: under sodium sulphite exists, in reactor, there is oxidizing reaction in a diisopropyl benzene and the oxygen continuing to pass into, the reaction times is 50 minutes, thus obtains dicumyl peroxide at 30 DEG C; Then add the aqueous hydrochloric acid that appropriate mass percent concentration is 15%, fully stir, obtain intermediate reaction product and acetone, and remove acetone;
Wherein the mass ratio of sodium sulphite and a diisopropyl benzene is 0.2:100;
S2: add in intermediate reaction product mass percent concentration be 25% formalin react, the reaction times is 6 hours, and temperature of reaction is 50 DEG C; React rear removing water layer, in residue system, then added equal-volume mixture and the water of acetone and ethanol, stir, obtain described crosslinker solution, by its called after JL1;
Between in formaldehyde in wherein said formalin and step S1, the mol ratio of diisopropyl benzene is 1:2;
The equal-volume mixture of described acetone and ethanol and the volume ratio of described residue system are 1:2.5;
The volume ratio of the equal-volume mixture of the water added and described acetone and ethanol is 1:2.
Crosslinker solution preparation example 2-7
Except replacing with except KOH, NaOH, sodium carbonate, sodium sulfate, salt of wormwood or sodium phosphate by the mineral alkali in crosslinker solution preparation example 1 respectively by sodium sulphite respectively, other operation is all constant, thus the corresponding crosslinker solution obtained, in turn called after JL2-JL7.
Ternary metal composite particles preparation example
(1) potassium chloride solution of the magnesium nitrate aqueous solution of 1mol/L, the aluminum sulfate aqueous solution of 1mmol/L and 1mmol/L is prepared respectively;
(2) in sodium phosphate aqueous solution, slowly add the NaOH aqueous solution, preparation NaOH concentration is 2mol/L and sodium phosphate concentration is the aqueous solution of 0.5mol/L;
(3) in the aqueous solution of step (2), add the magnesium nitrate aqueous solution of step (1), aluminum sulfate aqueous solution and potassium chloride solution in turn, after adding, Keep agitation 40 minutes, obtains reacting slurry; Wherein, the volume ratio of described magnesium nitrate aqueous solution, aluminum sulfate aqueous solution and potassium chloride solution is 2:1:2, and the volume ratio of the aqueous solution of the cumulative volume of these three kinds of aqueous solution and step (2) is 1:5;
(4) reacting slurry is left standstill slaking 4 hours at 110 DEG C, then naturally cools to room temperature, filter, deionized water fully wash 2-3 time, vacuum-drying, ground 300 mesh sieves, obtain described ternary metal composite particles, called after WL.
Modified alta-mud preparation example
I, wilkinite to be calcined 25 minutes at 550 DEG C, be then cooled to room temperature, and pulverize, grind, cross 300 mesh sieves, obtain wilkinite powder;
II, wilkinite powder, dimethyl dodecyl ammonium chloride and deionized water and stirring is even, react 150 minutes at 55 DEG C, then filter, vacuum-drying, obtain described modified alta-mud, called after PRT;
Wherein, the mass ratio of wilkinite powder, dimethyl dodecyl ammonium chloride and deionized water is 1:2:15.
Silicic acid many metal-salts preparation example 1
(I) to mass percent concentration be 2% sodium silicate aqueous solution in add the aqueous sulfuric acid that mass percent concentration is 15%, to regulate pH=4-5, then at room temperature stir 20 minutes, obtain acidic aqueous solution;
(II) in described acidic aqueous solution, add Tai-Ace S 150, zinc nitrate and titanium chloride, and stir, be then warming up to 50 DEG C with the temperature rise rate of 2 DEG C/min, stir 25 minutes at such a temperature; Be warming up to 70 DEG C with the temperature rise rate of 6 DEG C/min again, stir 15 minutes at such a temperature, finally leave standstill slaking 17 hours at such a temperature, drying, solidification, ground 300 mesh sieves, obtain the many metal-salts of described silicic acid, called after GS1.
Wherein, in step (II), the mol ratio of Tai-Ace S 150, zinc nitrate and titanium chloride is 1:1:2, and wherein the mole dosage sum of the three of aluminium element, zinc element and titanium elements is 4.5:1 with the ratio of the mole dosage of element silicon in water glass.
Silicic acid many metal-salts preparation example 2-3
Except in step (II) direct " being warming up to 50 DEG C with the temperature rise rate of 2 DEG C/min ", other operation is all same as silicic acid many metal-salts preparation example 1, namely direct at 50 DEG C the stirring reaction 40 minutes total reaction time of two differing temps intervals (in silicic acid many metal-salts preparation example 1), thus carried out silicic acid many metal-salts preparation example 2, by the silicic acid many metal-salts called after GS2 obtained.
Except in step (II) direct " being warming up to 70 DEG C with the temperature rise rate of 6 DEG C/min ", other operation is all same as silicic acid many metal-salts preparation example 1, namely direct at 70 DEG C the stirring reaction 40 minutes total reaction time of two differing temps intervals (in silicic acid many metal-salts preparation example 1), thus carried out silicic acid many metal-salts preparation example 3, by the silicic acid many metal-salts called after GS3 obtained.
Embodiment 1
(1) (its molecular weight is 2,400 ten thousand to take the partially hydrolyzed polyacrylamide of 0.2 weight part respectively, degree of hydrolysis be 25% and solid content be 98%), 0.3 weight part crosslinker solution JL1, 0.04 weight part ternary metal composite particles WL, 0.02 weight part promotor (is the mixture of potassiumphosphate and Sodium salts humic acids, both mass ratioes are 1:2), 0.08 weight part additive 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid four sodium, 0.04 part by weight modified wilkinite PRT, 0.08 weight part auxiliary agent ethoxyl methyl cellulose ether, 0.1 weight part complexing agent nitrilotriacetic acid(NTA), 0.05 weight part silicic acid many metal-salts GS1 and 20 weight parts waters,
(2) in described water, add whole partially hydrolyzed polyacrylamides successively, be the crosslinker solution (i.e. 0.18 weight part) of total weight parts 60%, whole ternary metal composite particles, whole promotor, whole additives, whole modified alta-muds, whole auxiliary agents, whole complexing agents and the many metal-salts of whole silicic acid, and stirring reaction 50 minutes, obtain pre-gathering solutions;
(3) in described pre-gathering solutions, add the crosslinker solution (i.e. 0.12 weight part) of residue 40%, and continue stirring reaction 20 minutes, obtain environmental protection organic profile control agent of the present invention, called after TPJ1.
Embodiment 2
(1) (its molecular weight is 2,450 ten thousand to take the partially hydrolyzed polyacrylamide of 1 weight part respectively, degree of hydrolysis be 27% and solid content be 98%), 0.6 weight part crosslinker solution JL1, 0.05 weight part ternary metal composite particles WL, 0.06 weight part promotor (is the mixture of potassiumphosphate and Sodium salts humic acids, both mass ratioes are 1:2), 0.1 weight part additive 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid four sodium, 0.07 part by weight modified wilkinite PRT, 0.15 weight part auxiliary agent hydroxypropyl methyl cellulose ether, 0.14 weight part complexing agent nitrilotriacetic acid(NTA), 0.09 weight part silicic acid many metal-salts GS1 and 40 weight parts waters,
(2) in described water, add whole partially hydrolyzed polyacrylamides successively, be the crosslinker solution (i.e. 0.48 weight part) of total weight parts 80%, whole ternary metal composite particles, whole promotor, whole additives, whole modified alta-muds, whole auxiliary agents, whole complexing agents and the many metal-salts of whole silicic acid, and stirring reaction 70 minutes, obtain pre-gathering solutions;
(3) in described pre-gathering solutions, add the crosslinker solution (i.e. 0.12 weight part) of residue 20%, and continue stirring reaction 30 minutes, obtain environmental protection organic profile control agent of the present invention, called after TPJ2.
Embodiment 3
(1) (its molecular weight is 2,400 ten thousand to take the partially hydrolyzed polyacrylamide of 1.5 weight parts respectively, degree of hydrolysis be 26% and solid content be 98%), 0.8 weight part crosslinker solution JL1, 0.07 weight part ternary metal composite particles WL, 0.04 weight part promotor (is the mixture of potassiumphosphate and Sodium salts humic acids, both mass ratioes are 1:2), 0.12 weight part additive 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid four sodium, 0.1 part by weight modified wilkinite PRT, 0.12 weight part auxiliary agent ethoxyl methyl cellulose ether, 0.12 weight part complexing agent nitrilotriacetic acid(NTA), 0.07 weight part silicic acid many metal-salts GS1 and 30 weight parts waters,
(2) in described water, add whole partially hydrolyzed polyacrylamides successively, be the crosslinker solution (i.e. 0.56 weight part) of total weight parts 70%, whole ternary metal composite particles, whole promotor, whole additives, whole modified alta-muds, whole auxiliary agents, whole complexing agents and the many metal-salts of whole silicic acid, and stirring reaction 60 minutes, obtain pre-gathering solutions;
(3) in described pre-gathering solutions, add the crosslinker solution (i.e. 0.24 weight part) of residue 30%, and continue stirring reaction 40 minutes, obtain environmental protection organic profile control agent of the present invention, called after TPJ3.
Embodiment 4-9
Except using following different crosslinker solutions respectively and replacing the crosslinker solution JL1 in embodiment 1-3, implement embodiment 4-9 respectively in the mode identical with embodiment 1-3, its respective enforcement corresponding relation, the name of gained amendment are as shown in the table:
Embodiment 10-15
Embodiment 10-12: except respectively additive wherein being replaced with except Amino Trimethylene Phosphonic Acid four sodium by 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid four sodium, other operation is all constant, thus respectively to implement embodiment 10-12 with the same way of embodiment 1-3, gained amendment is called after TPJ10-TPJ12 in turn.
Embodiment 13-15: except respectively additive wherein being replaced with except ethylene diamine tetra methylene phosphonic acid five sodium by 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid four sodium, other operation is all constant, thus respectively to implement embodiment 13-15 with the same way of embodiment 1-3, gained amendment is called after TPJ13-TPJ15 in turn.
Embodiment 16-20
Except using following different complexing agents respectively and replacing the complexing agent nitrilotriacetic acid(NTA) in embodiment 1-3, implement embodiment 16-20 respectively in the mode identical with embodiment 1-3, its respective enforcement corresponding relation, the name of gained amendment are as shown in the table:
Embodiment 21-26
Embodiment 21-23: except replacing with except GS2 by many for silicic acid wherein metal-salts by GS1 respectively, other operation is all constant, thus respectively to implement embodiment 21-23 with the same way of embodiment 1-3, gained amendment is called after TPJ21-TPJ23 in turn.
Embodiment 24-26: except replacing with except GS3 by many for silicic acid wherein metal-salts by GS1 respectively, other operation is all constant, thus respectively to implement embodiment 24-26 with the same way of embodiment 1-3, gained amendment is called after TPJ24-TPJ26 in turn.
Embodiment 27-45
Except the partially hydrolyzed polyacrylamide using following different piece hydro-polyacrylamide to replace in embodiment 1-3 respectively, implement embodiment 27-45 in the mode identical with embodiment 1-3 respectively, its molecular weight, degree of hydrolysis and solid content separately, enforcement corresponding relation, the name of gained amendment are as shown in the table:
Embodiment 46-48
Except the unmodified wilkinite of use replaces modified alta-mud of the present invention, other operation is all constant, and respectively to have carried out embodiment 46-48 with the same way of embodiment 1-3, the amendment obtained is called after TPJ46-TPJ48 in turn.
performance test
1, sealing ratiod is measured
Carry out the mensuration of sealing ratiod in accordance with the following steps:
Get fill out sand tube, the thermostat container putting into 60 DEG C heats 2 hours, surveys its rate of permeation (before injecting rate of permeation) with the conventional measuring method in this area; Then by amendment of the present invention according to 0.3ml/ minute/cm
2speed carry out injecting (every cm wherein
2for the sectional area of fill out sand tube, lower same), injection pressure is 0.09MPa, inject after 5 hours, stop injecting, and then measure rate of permeation (inject after rate of permeation), thus its sealing ratiod (sealing ratiod (%)=(before injecting after rate of permeation-injections rate of permeation)/inject front rate of permeation × 100%) can be calculated according to the rate of permeation of front and back twice, concrete outcome sees the following form:
As seen from the above table,
1, when mineral alkali used when prepared by crosslinker solution is different, certain influence can be produced to the sealing characteristics of the finished product.Wherein, sodium sulphite has best effect.
2, when changing the kind of additive and complexing agent, also plugging effect is made a significant impact.Wherein, 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid four sodium and nitrilotriacetic acid(NTA) are optimum additive and complexing agent, and the additive of other kind and complexing agent all cause sealing characteristics decrease to some degree.
In the preparation method of 3, many metal-salts of silicic acid, two-stage process heats up can have best technique effect.
In the selection of 4, the molecular weight of partially hydrolyzed polyacrylamide, degree of hydrolysis and solid content, molecular weight is 2400-2450 ten thousand, degree of hydrolysis is 25-27% and solid content is 98% have best plugging effect.
5, when not carrying out modification like this of the present invention to wilkinite, the significant reduction that caused plugging effect to have.
2, abrasion resistance is measured
Get fill out sand tube, the thermostat container putting into 60 DEG C heats 2 hours, surveys its rate of permeation (before injecting rate of permeation) with the conventional measuring method in this area; Then by amendment of the present invention according to 0.3ml/ minute/cm
2speed inject, injection pressure is 0.09MPa, injects after 5 hours, stop inject.Then wait solidifying 48 hours, finally carrying out displacement with deionized water, is 30 times of fill out sand tube volumes (namely washing away 30 times) by the deionized water volume of fill out sand tube, then calculates the final sealing ratiod after washing away, the results are shown in following table.
As seen from the above table, amendment of the present invention is after washing away 30 times, still there is good final sealing ratiod, but wherein TPJ1-TPJ3 has best abrasion resistance, when any one component changed wherein or wilkinite do not carry out modification and some treatment step changes to some extent, abrasion resistance is all caused to decrease.
3, heat resistance
Step 1: amendment of the present invention is measured respective filter loss after obtained under room temperature, and be then placed in seal pot respectively, valve-off, be in sealed state, then heat rolls 25 hours at 180 DEG C;
Step 2: after heat is rolled and is disposed, Open valve, naturally place and be cooled to room temperature, then the well control fluid after heat being rolled is placed to room temperature naturally, then the filter loss after pyroprocessing like this is measured, contrast with filter loss when not experiencing pyroprocessing in step 1, thus its durability performance can be investigated.
Wherein, the measuring method of filter loss belongs to very known routine techniques, and this is no longer going to repeat them.
The results are shown in following table.
As seen from the above table, the filter loss of TPJ1-TPJ3 after pyroprocessing is wanted significantly lower than before pyroprocessing, this demonstrate that TPJ1-TPJ3 has good high temperature resistant property (can meet the high temperature of 180 DEG C under application requiring).And when changing constituent species wherein and when some component not processed to (as wilkinite) or change some parameter (mineral alkali in the different or crosslinker solution preparation process of the physical property as partially hydrolyzed polyacrylamide is selected different), all will the filter loss after pyroprocessing be caused to enlarge markedly, demonstrate durability performance and will be weaker than TPJ1-TPJ3.
Add the selection on opportunity to investigate crosslinker solution in amendment preparation method of the present invention, thus carry out following comparative example.
Comparative example 1-6
Comparative example 1-3: add except whole crosslinker solution except disposable in step (2), other operation is all identical, thus respectively to have carried out comparative example 1-3 with the identical embodiment of embodiment 1-3, by gained amendment called after D1-D3 in turn.
Comparative example 4-6: add except whole crosslinker solution except disposable in step (3), other operation is all identical, thus respectively to have carried out comparative example 4-6 with the identical embodiment of embodiment 1-3, by gained amendment called after D4-D6 in turn.
According to above-mentioned same test method, seal-off effect, abrasion resistance and high temperature resistance are carried out to D1-D6 and measures, for the ease of comparing, and listing the data of TPJ1-TPJ48 in the lump, the results are shown in following table.
As can be seen here, it is fashionable when crosslinker solution is added in batches, all cause variously having remarkable reduction, it even will be significantly higher than the change of component and bentonitic unmodified etc. to sealing ratiod, abrasion resistance and durothermic impact, this proves in this preparation method, and adding in batches of crosslinker solution has obtained conclusive impact for final excellent effect.
As mentioned above, the invention provides a kind of organic profile control agent and preparation method thereof and purposes in the oil industry, this amendment is by the suitable selection of each component, the Particular craft etc. of preparation method, thus achieve each the most excellent performance, not only can realize the function of water blockoff, and there are good abrasion resistance, temperature tolerance etc., thus have a good application prospect and industrialization potential in petroleum industry field.
Should be appreciated that the purposes of these embodiments is only not intended to for illustration of the present invention limit the scope of the invention.In addition; also should understand; after having read technology contents of the present invention, those skilled in the art can make various change, amendment and/or modification to the present invention, and these all equivalent form of values fall within the protection domain that the application's appended claims limits equally.
Claims (10)
1. an environmental protection organic profile control agent, described amendment comprises partially hydrolyzed polyacrylamide, crosslinker solution, ternary metal composite particles, promotor, additive, modified alta-mud, auxiliary agent, complexing agent, the many metal-salts of silicic acid and water.
2. environmental protection organic profile control agent as claimed in claim 1, it is characterized in that: in described environmental protection organic profile control agent, with parts by weight, its concrete component concentration is as follows:
3. the environmental protection organic profile control agent as described in any one of claim 1-2, is characterized in that: described partially hydrolyzed polyacrylamide is anion-polyacrylamide, and its molecular weight is 2,000 ten thousand-2,800 ten thousand, degree of hydrolysis is 20-30% and solid content is 97-99%; Most preferably its molecular weight is 2400-2450 ten thousand, degree of hydrolysis be 25-27% and solid content is 98%.
4. the environmental protection organic profile control agent as described in any one of claim 1-3, is characterized in that: described crosslinker solution prepares according to the method comprised the steps:
S1: in the presence of an inorganic base, in reactor, a diisopropyl benzene and oxygen generation oxidizing reaction, obtain dicumyl peroxide; Then add acid, fully stir, obtain intermediate reaction product and acetone, removing acetone;
S2: add formalin in intermediate reaction product, react, has reacted rear removing water layer, then in residue system, adds organic solvent and water, stirs, obtain described crosslinker solution.
5. the environmental protection organic profile control agent as described in any one of claim 1-4, is characterized in that: described ternary metal composite particles prepares according to the method comprised the steps:
(1) potassium chloride solution of the magnesium nitrate aqueous solution of 1mol/L, the aluminum sulfate aqueous solution of 1mmol/L and 1mmol/L is prepared respectively;
(2) in sodium phosphate aqueous solution, slowly add the NaOH aqueous solution, preparation NaOH concentration is 2mol/L and sodium phosphate concentration is the aqueous solution of 0.5mol/L;
(3) in the aqueous solution of step (2), add the magnesium nitrate aqueous solution of step (1), aluminum sulfate aqueous solution and potassium chloride solution in turn, after adding, Keep agitation 30-50 minute, obtains reacting slurry;
(4) by reacting slurry at 100-120 DEG C leave standstill slaking 3-4 hour, then naturally cool to room temperature, filter, deionized water fully wash 2-3 time, vacuum-drying, ground 300 mesh sieves, obtain described ternary metal composite particles.
6. the environmental protection organic profile control agent as described in any one of claim 1-5, is characterized in that: described additive is Amino Trimethylene Phosphonic Acid four sodium, 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid four sodium or ethylene diamine tetra methylene phosphonic acid five sodium, most preferably is 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid four sodium.
7. the environmental protection organic profile control agent as described in any one of claim 1-6, is characterized in that: described modified alta-mud prepares according to the method comprised the steps:
I, wilkinite is calcined 20-30 minute at 500-600 DEG C, be then cooled to room temperature, and pulverize, grind, cross 300 mesh sieves, obtain wilkinite powder;
II, wilkinite powder, dimethyl dodecyl ammonium chloride and deionized water and stirring is even, at 50-60 DEG C, react 2-3 hour, then filter, vacuum-drying, obtain described modified alta-mud.
8. the environmental protection organic profile control agent as described in any one of claim 1-7, is characterized in that: the many metal-salts of described silicic acid prepare according to the method comprised the steps:
(I) to mass percent concentration be 1-2% sodium silicate aqueous solution in add the aqueous sulfuric acid that mass percent concentration is 10-20%, to regulate pH=4-5, then at room temperature stir 10-20 minute, obtain acidic aqueous solution;
(II) in described acidic aqueous solution, add Tai-Ace S 150, zinc nitrate and titanium chloride, and stir, be then warming up to 45-55 DEG C with the temperature rise rate of 2 DEG C/min, stir 20-30 minute at such a temperature; Be warming up to 65-80 DEG C with the temperature rise rate of 6 DEG C/min again, stir 10-15 minute at such a temperature, finally leave standstill slaking 15-20 hour at such a temperature, drying, solidification, ground 300 mesh sieves, obtain the many metal-salts of described silicic acid.
9. the preparation method of the environmental protection organic profile control agent described in any one of claim 1-8, described method comprises the steps:
(1) partially hydrolyzed polyacrylamide of respective weight part, crosslinker solution, ternary metal composite particles, promotor, additive, modified alta-mud, auxiliary agent, complexing agent, the many metal-salts of silicic acid and water is taken respectively;
(2) Xiang Shuizhong adds partially hydrolyzed polyacrylamide, crosslinker solution for total weight parts 60-80%, ternary metal composite particles, promotor, additive, modified alta-mud, auxiliary agent, complexing agent and the many metal-salts of silicic acid successively, and stirring reaction 50-70 minute, obtain pre-gathering solutions;
(3) in described pre-gathering solutions, add the crosslinker solution of residuals weight part, and continue stirring reaction 20-40 minute, obtain environmental protection organic profile control agent of the present invention.
10. the purposes of environmental protection organic profile control agent in oil production described in any one of claim 1-8.
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